CN104332214A - Low-temperature curing conductive silver paste and preparation method thereof - Google Patents
Low-temperature curing conductive silver paste and preparation method thereof Download PDFInfo
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- CN104332214A CN104332214A CN201410587410.0A CN201410587410A CN104332214A CN 104332214 A CN104332214 A CN 104332214A CN 201410587410 A CN201410587410 A CN 201410587410A CN 104332214 A CN104332214 A CN 104332214A
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Abstract
Low-temperature curing conductive silver paste comprises, in weight percent, 60-80% of silver powder, 5-20% of polymer resin carriers, 5-20% of epoxy resin low polymer, 5-10% of solvents and 0.1-5% of curing agents. A method for preparing the conductive silver paste includes the steps: firstly, preparing pre-polymer; secondly, preparing diffusers; thirdly, preparing precursor; finally, adding the silver powder into a stirring box, mixing the silver powder and then grinding and filtering the mixture to obtain the conductive silver paste. The low-temperature curing conductive silver paste can achieve low-temperature curing effects, and has excellent adhesive force and hardness.
Description
Technical field
The present invention relates to a kind of low-temperature cured conductive paste and preparation method thereof.
Background technology
At present, the development that electronics industry is being advanced by leaps and bounds, and conductive silver paste is the critical function material preparing electronic devices and components, current electrocondution slurry is mainly divided into thin film switch, capacitance plate, touch screens, solar energy slurry.Be divided into again low-temperature solidified silver paste, intermediate temperature setting silver slurry, high-temperature sintered silver paste according to condition of cure, conductive silver paste for touch screens is mainly low-temperature solidified silver paste.First low-temperature solidified silver paste will meet low temperature and can solidify, and after solidification, conductivity, adhesive force, hardness, environmental stability meet the requirements.
Current touch-screen low-temperature solidified silver paste mostly is imported product, is also short of to some extent in the domestic silver slurry all met the demands in preparation conductivity, adhesive force, hardness etc.Therefore, high conductivity, adhesive force and hardness all more excellent, the research and development of low-temperature solidified silver paste of continuous printing can cause extensive concern in the industry.
Summary of the invention
The technical problem to be solved in the present invention is, for the defect of conductive silver paste adhesive force of the prior art and hardness deficiency, provides a kind of low-temperature cured conductive silver slurry.
The technical solution adopted for the present invention to solve the technical problems is: construct a kind of low-temperature cured conductive
Silver slurry, this conductive silver paste is made up of the component of following mass percentage content:
Silver powder: 60 ~ 80;
Macromolecule resin carrier: 5 ~ 20;
Epoxy resin oligomer: 5 ~ 20;
Solvent: 5 ~ 10;
Curing agent: 0.1 ~ 5.
In low-temperature cured conductive silver slurry of the present invention, this conductive silver paste is by following percent mass
Make than the component of content:
Silver powder: 65 ~ 75;
Macromolecule resin carrier: 10 ~ 15;
Epoxy resin oligomer: 10 ~ 15;
Solvent: 6 ~ 8;
Curing agent: 1 ~ 3.
In low-temperature cured conductive silver slurry of the present invention, this conductive silver paste is by following percent mass
Make than the component of content:
Silver powder: 70;
Macromolecule resin carrier: 10;
Epoxy resin oligomer: 11;
Solvent: 7;
Curing agent: 2.
In low-temperature cured conductive silver slurry of the present invention, the average grain diameter of described silver powder is 1.0 ~ 5.0 microns, and specific area is 1.0 ~ 2.2 meters squared per gram, and the purity of silver powder is greater than 99.95%.
In low-temperature cured conductive silver slurry of the present invention, described macromolecule resin carrier is HMW polyurethane resin, and its molecular weight is greater than 100000, and its glass transition temperature is greater than 50 DEG C.
In low-temperature cured conductive silver slurry of the present invention, described solvent is high boiling solvent, and it is the one in different fluorine that ketone, naphtha, two ethanedioic acid ethyl ether acetate esters, diethylene adipate, ethanedioic acid ethyl ether acetate ester, ethanedioic acid monobutyl ether acetate, DBE.
In low-temperature cured conductive silver slurry of the present invention, described curing agent is epoxy hardener, and it is the one in isocyanates, imidazoles, dicyandiamide.
Another technical problem that the present invention will solve is, for the defect of conductive silver paste adhesive force of the prior art and hardness deficiency, provides a kind of method preparing low-temperature cured conductive silver slurry.
The present invention solves the technical scheme that its another technical problem adopts: construct a kind of method preparing low-temperature cured conductive silver slurry, it is characterized in that, comprise the following steps:
Take by each component of conductive silver paste described in claims 1 to 3; First prepare performed polymer:
S1 adds epoxy resin and curing agent successively in stirring box, and stir 1 minute with stirring defoamer, then deaeration is after 1 minute; Add isocyanates wherein again, again stir 1 minute, gained mixture, after 1 minute, is transferred in there-necked flask by deaeration;
S2 puts into hot-air oven by after the sealing of above-mentioned there-necked flask, takes out after completion of the reaction, is transferred to by the epoxy oligomer obtained to put into refrigerator 5 ~ 10 DEG C of refrigerations after sealing in sample bottle and deposit, for subsequent use.
Prepare in the method for low-temperature cured conductive silver slurry of the present invention, also comprise the step of preparation dispersion:
S3 adds solvent by flask, then adds macromolecule resin particle, stir 4 little after resin disperses completely, and take out be transferred in described sample bottle, in the airtight preservation of room temperature, for subsequent use;
In the method preparing low-temperature cured conductive silver slurry of the present invention, also comprise the step preparing presoma:
S4 gets described dispersion and described epoxy oligomer in stirring box, and adds catalyst, stirs 1 minute, then deaeration 1 minute, obtains presoma, deposits in 5 ~ 10 DEG C of refrigerations, for subsequent use;
S5 gets above-mentioned presoma, and adds silver powder in described stirring box, after mixing, through grinding, filters, namely obtains the conductive silver paste described in claims 1 to 3.
Low-temperature cured conductive silver slurry slurry of the present invention can reach low-temperature setting effect, and adhesive force and hardness excellence.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
Silver powder: apparent density 0.8-1.7g/ml; Tap density 2.5-3.5g/ml, average grain diameter is 1.0-4.0um; Specific area is less than 2m
2/ g; Burn out rate (550 DEG C, 0.5h) is less than 1%; Silver purity more than 99.95%.
Epoxy resin oligomer: mainly comprise isocyanates 15-25%, imidazoles epoxy hardener 0.5-5%, epoxy resin 70-80%, obtain at 70-120 DEG C of reaction 0.5-4h after three's mixing, the percentage by weight that described epoxy resin oligomer accounts for silver-colored slurry system is 25-35%.
Solvent: the one in different fluorine that ketone, naphtha, two ethanedioic acid ethyl ether acetate esters, diethylene adipate, ethanedioic acid ethyl ether acetate ester, ethanedioic acid monobutyl ether acetate, DBE, weight ratio is 5-10% in silver-colored slurry system.
Curing agent: be the one in isocyanates, imidazoles, dicyandiamide, percentage by weight is the 0.1-5% of system.
Macromolecule resin carrier is that HMW polyurethane resin has excellent mechanical performance, and molecular weight is greater than 100000, glass transition temperature >50 DEG C, and mass ratio is 5-10%.
Take silver powder 259g, different fluorine that ketone 40g, epoxy resin oligomer 25g, isocyanates 0.3g, HMW polyurethane resin 15g.
Prepare performed polymer:
S1 adds epoxy resin oligomer 25g and catalyst successively in stirring box, stirs defoamer with Thinky() stir 1 minute, then deaeration is after 1 minute; Add isocyanates 0.3g wherein again, again stir 1 minute, gained mixture, after 1 minute, is transferred in there-necked flask by deaeration;
S2 puts into hot-air oven by after the sealing of above-mentioned there-necked flask, takes out after completion of the reaction, the epoxy resin oligomer obtained is transferred to put into refrigerator 5-10 DEG C refrigeration after sealing in sample bottle and deposit, for subsequent use;
Preparation dispersion:
S3 will add different fluorine that ketone 40g in flask, then adds HMW urethane resin particles 15g, stirs 4 hours, disperses rear taking-up to be transferred in sample bottle completely to resin, the airtight preservation of room temperature, for subsequent use;
Prepare presoma:
S4 gets the above-mentioned dispersion for preparing and epoxy oligomer in stirring box, and adds catalyst, stir 1 minute, then deaeration is after 1 minute, obtains presoma, deposits in 5-10 DEG C of refrigeration, for subsequent use;
Preparation silver slurry:
Get above-mentioned presoma, and add 259g silver powder in stirring box, after mixing, grinding, filters, namely obtains conductive silver paste.
According to the conductive silver paste that the present embodiment 1 is obtained, its performance is as follows:
Curing temperature: 130 DEG C, 1h,
Resistivity≤7*10-5 Ω .cm,
Adhesive force: 5B is without coming off;
Hardness: H
Constant temperature and humidity test: 85 DEG C of 80% humidity repetition measurement adhesive force 5B without coming off, hardness H, change in resistance <15%.
Embodiment 2
Silver powder: apparent density 0.8-1.7g/ml; Tap density 2.5-3.5g/ml, average grain diameter is 1.0-4.0um; Specific area is less than 2m
2/ g; Burn out rate (550 DEG C, 0.5h) is less than 1%; Silver purity more than 99.95%.
Epoxy resin oligomer: mainly comprise isocyanates 15-25%, imidazoles epoxy hardener 0.5-5%, epoxy resin 70-80%, obtain at 70-120 DEG C of reaction 0.5-4h after three's mixing, the percentage by weight that described epoxy resin oligomer accounts for silver-colored slurry system is 25-35%.
Solvent: the one in different fluorine that ketone, naphtha, two ethanedioic acid ethyl ether acetate esters, diethylene adipate, ethanedioic acid ethyl ether acetate ester, ethanedioic acid monobutyl ether acetate, DBE, weight ratio is 5-10% in silver-colored slurry system.
Curing agent: be the one in isocyanates, imidazoles, dicyandiamide, percentage by weight is the 0.1-5% of system.
Macromolecule resin carrier is that HMW polyurethane resin has excellent mechanical performance, and molecular weight is greater than 100000, glass transition temperature >50 DEG C, and mass ratio is 5-10%.
Take silver powder 259g, ethanedioic acid monobutyl ether acetate 45g, epoxy resin oligomer 30g, dicyandiamide 0.3g, HMW polyurethane resin 15g.
Prepare performed polymer:
S1 adds epoxy resin oligomer 30g and catalyst successively in stirring box, stirs defoamer with Thinky() stir 1 minute, then deaeration is after 1 minute; Add dicyandiamide 0.3g wherein again, again stir 1 minute, gained mixture, after 1 minute, is transferred in there-necked flask by deaeration;
S2 puts into hot-air oven by after the sealing of above-mentioned there-necked flask, takes out after completion of the reaction, the epoxy resin oligomer obtained is transferred to put into refrigerator 5-10 DEG C refrigeration after sealing in sample bottle and deposit, for subsequent use;
Preparation dispersion:
S3 will add ethanedioic acid monobutyl ether acetate 45g in flask, then adds HMW urethane resin particles 15g, stirs 4 hours, disperses rear taking-up to be transferred in sample bottle completely to resin, and the airtight preservation of room temperature is for subsequent use;
Prepare presoma:
S4 gets the above-mentioned dispersion for preparing and epoxy resin oligomer in stirring box, and adds catalyst, stir 1 minute, then deaeration is after 1 minute, obtains presoma, deposits in 5-10 DEG C of refrigeration, for subsequent use;
Preparation silver slurry:
Get above-mentioned presoma, and add 259g silver powder in stirring box, after mixing, grinding, filters, namely obtains conductive silver paste.
According to the conductive silver paste that the present embodiment 2 is obtained, its performance is as follows:
Curing temperature: 130 DEG C, 1h,
Resistivity≤7*10-5 Ω .cm,
Adhesive force: 5B is without coming off;
Hardness: H
Constant temperature and humidity test: 85 DEG C of 80% humidity repetition measurement adhesive force 5B without coming off, hardness H, change in resistance <15%.
Embodiment 3
Silver powder: apparent density 0.8-1.7g/ml; Tap density 2.5-3.5g/ml, average grain diameter is 1.0-4.0um; Specific area is less than 2m2/g; Burn out rate (550 DEG C, 0.5h) is less than 1%; Silver purity more than 99.95%.
Epoxy resin oligomer: mainly comprise isocyanates 15-25%, imidazoles epoxy hardener 0.5-5%, epoxy resin 70-80%, obtain at 70-120 DEG C of reaction 0.5-4h after three's mixing, the percentage by weight that described epoxy resin oligomer accounts for silver-colored slurry system is 25-35%.
Solvent: the one in different fluorine that ketone, naphtha, two ethanedioic acid ethyl ether acetate esters, diethylene adipate, ethanedioic acid ethyl ether acetate ester, ethanedioic acid monobutyl ether acetate, DBE, weight ratio is 5-10% in silver-colored slurry system.
Curing agent: be the one in isocyanates, imidazoles, dicyandiamide, percentage by weight is the 0.1-5% of system.
Macromolecule resin carrier is that HMW polyurethane resin has excellent mechanical performance, and molecular weight is greater than 100000, glass transition temperature >50 DEG C, and mass ratio is 5-10%.
Take silver powder 259g, diethylene adipate 35g, epoxy resin oligomer 30g, imidazoles 0.3g, HMW polyurethane resin 16g.
Prepare performed polymer:
S1 adds epoxy resin oligomer 30g and catalyst successively in stirring box, stirs defoamer with Thinky() stir 1 minute, then deaeration is after 1 minute; Add imidazoles 0.3g wherein again, again stir 1 minute, gained mixture, after 1 minute, is transferred in there-necked flask by deaeration;
S2 puts into hot-air oven by after the sealing of above-mentioned there-necked flask, takes out after completion of the reaction, the epoxy resin oligomer obtained is transferred to put into refrigerator 5-10 DEG C refrigeration after sealing in sample bottle and deposit, for subsequent use;
Preparation dispersion:
S3 will add diethylene adipate 35g in flask, then adds HMW urethane resin particles 16g, stirs 4 hours, disperses rear taking-up to be transferred in sample bottle completely to resin, and the airtight preservation of room temperature is for subsequent use;
Prepare presoma:
S4 gets the above-mentioned dispersion for preparing and epoxy resin oligomer in stirring box, and adds catalyst, stir 1 minute, then deaeration is after 1 minute, obtains presoma, deposits in 5-10 DEG C of refrigeration, for subsequent use;
Prepare conductive silver paste:
Get above-mentioned presoma, and add 259g silver powder in stirring box, after mixing, grinding, filters, namely obtains conductive silver paste.
According to the conductive silver paste that the present embodiment 3 is obtained, its performance is as follows:
Curing temperature: 130 DEG C, 1h,
Resistivity≤7*10-5 Ω .cm,
Adhesive force: 5B is without coming off;
Hardness: H
Constant temperature and humidity test: 85 DEG C of 80% humidity repetition measurement adhesive force 5B without coming off, hardness H, change in resistance <15%.
Low-temperature cured conductive silver slurry of the present invention can reach low-temperature setting effect, and adhesive force and hardness excellence.
Although by above embodiment to invention has been announcement, protection scope of the present invention is not limited thereto, under the condition not departing from the present invention's design, all will fall in right of the present invention the distortion, replacement etc. that above each component does.
Claims (10)
1. a low-temperature cured conductive silver slurry, it is characterized in that, this conductive silver paste is by following quality hundred
The component of proportion by subtraction content is made:
Silver powder: 60 ~ 80;
Macromolecule resin carrier: 5 ~ 20;
Epoxy resin oligomer: 5 ~ 20;
Solvent: 5 ~ 10;
Curing agent: 0.1 ~ 5.
2. low-temperature cured conductive silver slurry as claimed in claim 1, is characterized in that, this conductive silver paste
Be made up of the component of following mass percentage content:
Silver powder: 65 ~ 75;
Macromolecule resin carrier: 10 ~ 15;
Epoxy resin oligomer: 10 ~ 15;
Solvent: 6 ~ 8;
Curing agent: 1 ~ 3.
3. low-temperature cured conductive silver slurry as claimed in claim 1, is characterized in that, this conductive silver paste
Be made up of the component of following mass percentage content:
Silver powder: 70;
Macromolecule resin carrier: 10;
Epoxy resin oligomer: 11;
Solvent: 7;
Curing agent: 2.
4. low-temperature cured conductive silver is starched as claimed any one in claims 1 to 3, and it is characterized in that, the average grain diameter of described silver powder is 1.0 ~ 5.0 microns, and specific area is 1.0 ~ 2.2 meters squared per gram, and the purity of silver powder is greater than 99.95%.
5. low-temperature cured conductive silver is starched as claimed any one in claims 1 to 3, and it is characterized in that, described macromolecule resin carrier is HMW polyurethane resin, and its molecular weight is greater than 100000, and its glass transition temperature is greater than 50 DEG C.
6. low-temperature cured conductive silver is starched as claimed any one in claims 1 to 3, it is characterized in that, described solvent is high boiling solvent, and it is the one in different fluorine that ketone, naphtha, two ethanedioic acid ethyl ether acetate esters, diethylene adipate, ethanedioic acid ethyl ether acetate ester, ethanedioic acid monobutyl ether acetate, DBE.
7. low-temperature cured conductive silver is starched as claimed any one in claims 1 to 3, and it is characterized in that, described curing agent is epoxy hardener, and it is the one in isocyanates, imidazoles, dicyandiamide.
8. prepare a method for low-temperature cured conductive silver slurry, it is characterized in that, comprise the following steps:
Take by each component of conductive silver paste described in claims 1 to 3; First prepare performed polymer:
S1 adds epoxy resin and curing agent successively in stirring box, and stir 1 minute with stirring defoamer, then deaeration is after 1 minute; Add isocyanates wherein again, again stir 1 minute, gained mixture, after 1 minute, is transferred in there-necked flask by deaeration;
S2 puts into hot-air oven by after the sealing of above-mentioned there-necked flask, takes out after completion of the reaction, is transferred to by the epoxy oligomer obtained to put into refrigerator 5 ~ 10 DEG C of refrigerations after sealing in sample bottle and deposit, for subsequent use.
9. prepare the method for low-temperature cured conductive silver slurry as claimed in claim 8, it is characterized in that, also comprise the step of preparation dispersion:
S3 adds solvent by flask, then adds macromolecule resin particle, stir 4 little after resin disperses completely, and take out be transferred in described sample bottle, in the airtight preservation of room temperature, for subsequent use.
10. prepare the method for low-temperature cured conductive silver slurry as claimed in claim 9, it is characterized in that, also comprise the step preparing presoma:
S4 gets described dispersion and described epoxy oligomer in stirring box, and adds catalyst, stirs 1 minute, then deaeration 1 minute, obtains presoma, deposits in 5 ~ 10 DEG C of refrigerations, for subsequent use;
S5 gets above-mentioned presoma, and adds silver powder in described stirring box, after mixing, through grinding, filters, namely obtains the conductive silver paste described in claims 1 to 3.
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| CN201410587410.0A CN104332214B (en) | 2014-10-28 | A kind of low-temperature cured conductive silver slurry and preparation method thereof |
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| CN201410587410.0A CN104332214B (en) | 2014-10-28 | A kind of low-temperature cured conductive silver slurry and preparation method thereof |
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| CN104332214B CN104332214B (en) | 2017-01-04 |
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